This paper is devoted to the study of inverse problem of the permittivity and permeability tensor reconstruction of anisotropic materials in the form of diaphragms (sections) in a single-mode waveguide of rectangular cross section from the transmission and reflection coefficients measured. Results of numerical modeling are presented for different types of anisotropic materials. The developed solution techniques for the inverse problem under study can be applied in optics, nanotechnology, and design of microwave devices.